JP4918897B2 - Silicon single crystal pulling method - Google Patents
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- 229910052710 silicon Inorganic materials 0.000 title claims description 157
- 239000010703 silicon Substances 0.000 title claims description 157
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 156
- 239000013078 crystal Substances 0.000 title claims description 142
- 238000000034 method Methods 0.000 title claims description 43
- 239000007788 liquid Substances 0.000 claims description 72
- 230000005499 meniscus Effects 0.000 claims description 37
- 238000009826 distribution Methods 0.000 claims description 24
- 238000004033 diameter control Methods 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 11
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000003384 imaging method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims 1
- 230000004927 fusion Effects 0.000 description 39
- 230000007547 defect Effects 0.000 description 6
- 239000000155 melt Substances 0.000 description 4
- 229920005591 polysilicon Polymers 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010219 correlation analysis Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
- C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
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Description
本発明はチョクラルスキー法によりシリコン融液からシリコン単結晶を引上げる際に、シリコン単結晶の直径を的確に制御することによって、結晶欠陥の少ない高品質なシリコン単結晶を得ることが可能なシリコン単結晶引上方法に関する。 The present invention makes it possible to obtain a high-quality silicon single crystal with few crystal defects by accurately controlling the diameter of the silicon single crystal when pulling up the silicon single crystal from the silicon melt by the Czochralski method. The present invention relates to a silicon single crystal pulling method.
従来より、シリコン単結晶を製造するには種々の方法があるが、最も代表的なシリコン単結晶の製造方法としてチョクラルスキー法(以下、CZ法と称する)が挙げられる。このCZ法によるシリコン単結晶の育成では、ポリシリコンをルツボで溶解してシリコン融液を形成する。そして、このシリコン融液に種結晶を浸漬して、所定の回転速度、引上速度で種結晶を引き上げることによって、種結晶の下方に円柱状のシリコン単結晶が育成されるものである。 Conventionally, there are various methods for producing a silicon single crystal, and the most typical method for producing a silicon single crystal is the Czochralski method (hereinafter referred to as CZ method). In growing a silicon single crystal by this CZ method, polysilicon is melted with a crucible to form a silicon melt. Then, by immersing the seed crystal in this silicon melt and pulling up the seed crystal at a predetermined rotational speed and pulling speed, a cylindrical silicon single crystal is grown below the seed crystal.
半導体デバイスの材料となるシリコンウェーハは、このようなシリコン単結晶をスライス、研磨などを行うことによって得られる。こうしたシリコンウェーハの各種特性を一定レベル以上に保つためには、素材であるシリコン単結晶の育成時に、直胴部の直径が一定の範囲内になるように制御することが、製品品質ならびに製造費用の観点から極めて重要である。 A silicon wafer as a material for a semiconductor device can be obtained by slicing, polishing and the like of such a silicon single crystal. In order to keep these various characteristics of silicon wafers above a certain level, it is necessary to control the diameter of the straight body part within a certain range when growing the silicon single crystal material. From the viewpoint of
こうした、シリコン単結晶の育成時における直胴部の直径制御方法として、例えば、実際に引上げたシリコン単結晶の直径の計測値と、予め設定した直径の設定値とのズレ(差分)を算出し、シリコン融液の温度や引上速度にフィードバックして直径を制御することによって、シリコン単結晶の直径を予め設定した直径に近づけることが知られている(例えば、特許文献1,2参照)。 As a method for controlling the diameter of the straight body portion during the growth of the silicon single crystal, for example, a deviation (difference) between a measured value of the diameter of the actually pulled silicon single crystal and a preset value of the diameter is calculated. It is known that the diameter of a silicon single crystal is brought close to a preset diameter by controlling the diameter by feeding back to the temperature or pulling speed of the silicon melt (see, for example, Patent Documents 1 and 2).
しかし、上述したように、引上げられたシリコン単結晶の直径を測定してから、予め設定した直径の設定値とのズレを算出してフィードバックする方法では、シリコン単結晶の直径を精度よく制御することは困難であった。即ち、固液界面近傍に直径の測定位置を設定したとしても、既に引上げられたシリコン単結晶の直径にズレが検出された時点からシリコン融液の温度や引上速度を変化させたのでは、シリコン単結晶の実際の直径が設定値に近づくまでには相当の時間がかかる。このため、シリコン単結晶に直径の変動によるうねりが生じてしまい、シリコン単結晶の直胴部の直径を一定に保つことは難しい。 However, as described above, in the method in which the diameter of the pulled silicon single crystal is measured and then the deviation from the preset value of the diameter is calculated and fed back, the diameter of the silicon single crystal is accurately controlled. It was difficult. That is, even if the measurement position of the diameter is set near the solid-liquid interface, the temperature of the silicon melt and the pulling speed are changed from the time when the deviation is detected in the diameter of the already pulled silicon single crystal. It takes considerable time for the actual diameter of the silicon single crystal to approach the set value. For this reason, undulation due to the variation in diameter occurs in the silicon single crystal, and it is difficult to keep the diameter of the straight body portion of the silicon single crystal constant.
一方、シリコン単結晶の引上げ時に固液界面付近に生じる高輝度帯(フュージョンリングなどとも言う)を利用してシリコン単結晶の直径制御を行う方法も知られている(例えば、特許文献3参照)。この高輝度帯(フュージョンリング)は、引上中のシリコン単結晶の表面張力により持ち上がったシリコン融液の表面に、ルツボ壁からの放射光が反射して、固液界面でシリコン単結晶を取り巻く環状の高輝度領域が形成されたものである。こうした高輝度帯(フュージョンリング)を傾斜面とみなしてこの傾斜角度を継続して測定し、この高輝度帯における傾斜角度の変動を検出することにより、シリコン単結晶の直径の変化を検出するものである。 On the other hand, there is also known a method for controlling the diameter of a silicon single crystal by utilizing a high luminance band (also referred to as a fusion ring) generated near the solid-liquid interface when the silicon single crystal is pulled up (for example, see Patent Document 3). . This high-intensity band (fusion ring) surrounds the silicon single crystal at the solid-liquid interface by reflecting the radiation from the crucible wall to the surface of the silicon melt lifted by the surface tension of the silicon single crystal being pulled up. An annular high luminance region is formed. This high-intensity band (fusion ring) is regarded as an inclined surface, and this inclination angle is continuously measured, and changes in the inclination angle in this high-intensity band are detected to detect changes in the diameter of the silicon single crystal. It is.
また、ルツボからの放射光を抑制して、傾斜面とみなした高輝度帯(フュージョンリング)の外径あるいは幅を検出する構造も知られている(例えば、特許文献4参照)。 Also known is a structure that detects the outer diameter or width of a high-luminance zone (fusion ring) that is regarded as an inclined surface by suppressing the radiation light from the crucible (see, for example, Patent Document 4).
しかしながら、傾斜面とみなした高輝度帯(フュージョンリング)の角度や径寸法を検出し、これ基づいてシリコン単結晶の直径を制御する方法では、検出対象となる高輝度帯(フュージョンリング)の境界面が必ずしも明瞭ではなく、高輝度帯(フュージョンリング)の幅や直径を正確に検出することは困難である。従って、こうした高輝度帯(フュージョンリング)の幅や直径の変動をフィードバックさせてシリコン単結晶の直径を精度良く制御することは、困難であるのが現状であった。
本発明は上記課題を解決するためになされたものであり、チョクラルスキー法によりシリコン融液からシリコン単結晶を引上げる際に、シリコン単結晶の直径を正確に制御することによって、結晶欠陥の少ない高品質なシリコン単結晶を得ることが可能なシリコン単結晶引上方法を提供することを目的とする。 The present invention has been made in order to solve the above-mentioned problems, and when the silicon single crystal is pulled from the silicon melt by the Czochralski method, the diameter of the silicon single crystal is accurately controlled, so that the crystal defects are eliminated. An object of the present invention is to provide a silicon single crystal pulling method capable of obtaining a small number of high quality silicon single crystals.
上記課題を解決するために、本発明は次のようなシリコン単結晶引上方法を提供する。
すなわち、本発明のシリコン単結晶引上方法は、ルツボに収容した多結晶シリコンを溶融して前記ルツボにシリコン融液を形成する溶融工程と、チョクラルスキー法により前記シリコン融液からシリコン単結晶を引上げる引上工程とを有するシリコン単結晶引上方法であって、
前記引上工程において、撮像装置を用いて前記シリコン単結晶を撮像し、該撮像装置で撮像した画像中の前記シリコン融液と前記シリコン単結晶との固液界面近傍に生じる高輝度帯の輝度分布を各画像走査線毎に測定し、前記シリコン融液の液面位置と、前記固液界面位置とをそれぞれ検出する工程と、
前記液面位置と前記固液界面位置との差分であるメニスカス高さに基づいて、前記シリコン単結晶の直径制御を行う工程とを備え、
前記メニスカス高さは、前記画像中の固液界面近傍に生じる高輝度帯の前記各走査線毎の輝度分布において輝度が最も高い輝度ピーク部での検出位置を円近似し算出した中心位置による固液界面位置と、前記輝度ピーク部に対して前記シリコン融液側の輝度分布裾野部での位置を円近似し算出した中心位置による液面位置との差分であり、
前記液面位置を算出する際の輝度分布の裾野部分を前記輝度ピーク部の値に所定の閾値割合を乗算して求めた輝度閾値を用いて検出された位置とし、前記閾値割合は、70%以上90%以下の範囲であることを特徴とする。
本発明のシリコン単結晶引上方法は、ルツボに収容した多結晶シリコンを溶融して前記ルツボにシリコン融液を形成する溶融工程と、チョクラルスキー法により前記シリコン融液からシリコン単結晶を引上げる引上工程とを有するシリコン単結晶引上方法であって、
前記引上工程において、撮像装置を用いて前記シリコン単結晶を撮像し、撮像した画像中の前記シリコン融液と前記シリコン単結晶との固液界面近傍に生じる高輝度帯の、輝度分布を各画像走査線毎に測定し、前記シリコン融液の液面位置と、前記固液界面位置とをそれぞれ検出する工程と、
前記液面位置と前記固液界面位置との差分であるメニスカス高さに基づいて、前記シリコン単結晶の直径制御を行う工程とを備えたことを特徴とする。
In order to solve the above problems, the present invention provides the following silicon single crystal pulling method.
That is, the silicon single crystal pulling method of the present invention includes a melting step of melting polycrystalline silicon contained in a crucible to form a silicon melt in the crucible, and a silicon single crystal from the silicon melt by the Czochralski method. A silicon single crystal pulling method having a pulling step of pulling up,
In the pulling-up step, the silicon single crystal is imaged using an imaging device, and the brightness of a high-luminance zone generated in the vicinity of the solid-liquid interface between the silicon melt and the silicon single crystal in the image captured by the imaging device Measuring the distribution for each image scanning line, and detecting each of the liquid surface position of the silicon melt and the solid-liquid interface position;
A step of controlling the diameter of the silicon single crystal based on a meniscus height which is a difference between the liquid surface position and the solid-liquid interface position;
The meniscus height is a fixed value based on the center position calculated by circularly approximating the detection position at the luminance peak portion where the luminance is highest in the luminance distribution for each scanning line in the high luminance band generated near the solid-liquid interface in the image. The difference between the liquid interface position and the liquid surface position by the center position calculated by circularly approximating the position at the luminance distribution skirt part on the silicon melt side with respect to the luminance peak part,
The base part of the luminance distribution at the time of calculating the liquid surface position is a position detected by using a luminance threshold value obtained by multiplying the value of the luminance peak part by a predetermined threshold ratio, and the threshold ratio is 70% It is characterized by being in the range of 90% or less.
The silicon single crystal pulling method of the present invention includes a melting step in which polycrystalline silicon contained in a crucible is melted to form a silicon melt in the crucible, and a silicon single crystal is drawn from the silicon melt by the Czochralski method. A silicon single crystal pulling method having a pulling step to raise,
In the pulling-up step, the silicon single crystal is imaged using an imaging device, and each of the luminance distributions of the high luminance band generated in the vicinity of the solid-liquid interface between the silicon melt and the silicon single crystal in the captured image is displayed. Measuring each image scanning line, and detecting each of the liquid surface position of the silicon melt and the solid-liquid interface position;
And a step of controlling the diameter of the silicon single crystal based on a meniscus height that is a difference between the liquid surface position and the solid-liquid interface position.
このようなシリコン単結晶引上方法によれば、輝度測定手段によって高輝度帯(フュージョンリング)の、シリコン単結晶を引上方向に沿った輝度分布を各画像走査線毎に測定し、測定した輝度分布に基づいて、シリコン融液の液面位置と、固液界面位置とをそれぞれ検出する。そして、液面位置と固液界面位置との差分であるメニスカス高さの変動を連続して監視(測定)することによって、シリコン単結晶の直径が変動し始める兆候をいち早く検知して、シリコン単結晶の直径制御を迅速、かつ確実に行うことが可能になる。
ここで、フュージョンリングは、単結晶を中心とした曲面状をなしており、ほぼ円筒状である単結晶下端縁部から、水平面である融液面まで、結晶中心から放射状になだらかに変化する曲面となっている。本願発明では、このなだらかなフュージョンリグの結晶引上方向における寸法、すなわち、メニスカス高さの値を正確に測定して、この値の変化から、より精密な結晶径寸法制御が可能な引上方法を提供するものである。
According to such a silicon single crystal pulling method, the luminance measurement means measures the luminance distribution along the pulling direction of the silicon single crystal in the high luminance band (fusion ring) for each image scanning line. Based on the luminance distribution, the liquid surface position of the silicon melt and the solid-liquid interface position are detected. Then, by continuously monitoring (measuring) the fluctuation of the meniscus height, which is the difference between the liquid surface position and the solid-liquid interface position, the signs of the silicon single crystal starting to fluctuate are quickly detected, and the silicon single crystal is detected. It becomes possible to control the diameter of the crystal quickly and reliably.
Here, the fusion ring has a curved surface centered on the single crystal, and the curved surface gradually changes radially from the crystal center from the substantially cylindrical single crystal lower end edge to the melt surface which is a horizontal surface. It has become. In the present invention, the size of the gentle fusion rig in the crystal pulling direction, that is, the value of the meniscus height is accurately measured, and from this change in the pulling method, the crystal diameter can be controlled more precisely. Is to provide.
このように、シリコン単結晶の直径制御に、高輝度帯(フュージョンリング)の、シリコン単結晶を引上方向に沿った輝度分布を利用する方法は、従来のような、傾斜面とみなしてその形状が正確でない上、境界が明瞭でない高輝度帯(フュージョンリング)の傾斜角度や水平方向の径寸法である直径の変動を検出する方法と比較して、引上中のシリコン単結晶の直径の変化を正確、かつ迅速に検出することができる。
本発明のような、引上制御の正確性は、ドーナツ状の曲面の下内側4半分を切り取ったようなフュージョンリグをそのまま曲面として測定し、かつ、その引上方向における寸法、つまり、メニスカス高さを直径変動にかかるパラメータとして設定したことによって、はじめて実現されるものである。
As described above, the method of using the luminance distribution along the pulling direction of the silicon single crystal in the high luminance band (fusion ring) for the diameter control of the silicon single crystal is regarded as an inclined surface as in the conventional case. Compared to the method of detecting the tilt angle of the high-intensity zone (fusion ring) where the shape is inaccurate and the boundary is not clear and the variation of the diameter, which is the horizontal dimension, the diameter of the silicon single crystal being pulled is Changes can be detected accurately and quickly.
The accuracy of the pull-up control as in the present invention is measured by measuring a fusion rig obtained by cutting the lower inner four-half of a donut-shaped curved surface as a curved surface, and measuring the dimension in the pull-up direction, that is, the meniscus height. This is realized for the first time by setting the thickness as a parameter related to the diameter variation.
よって、シリコン単結晶の直径が予め設定した規定値よりも大幅にズレてしまう前に、シリコン単結晶の直径が予め設定した規定値内に収まるように、シリコン単結晶の引上速度および加熱ヒータの出力など、シリコン単結晶の直径制御に係る手段に対して、迅速にフィードバックすることが可能になる。これにより、直胴部の直径が一定に保たれた、結晶欠陥の少ない高品質なシリコン単結晶を得ることが可能になる。 Therefore, the pulling speed of the silicon single crystal and the heater are adjusted so that the diameter of the silicon single crystal falls within the preset specified value before the diameter of the silicon single crystal is significantly deviated from the preset specified value. It is possible to quickly feed back the means related to the diameter control of the silicon single crystal, such as the output of. Thereby, it is possible to obtain a high-quality silicon single crystal with few crystal defects, in which the diameter of the straight body portion is kept constant.
前記メニスカス高さは、液面位置と固液界面位置の差分であればよい。
具体的には、固液界面位置は前記高輝度帯(フュージョンリング)の輝度ピーク部での位置を円近似し算出した中心位置から求め、液面位置は前記高輝度帯(フュージョンリング)の輝度ピーク部より融液側の裾野部での位置を円近似し算出した中心位置から求める。メニスカス高さはその両者の差分となる。液面位置を算出する際に必要な高輝度帯(フュージョンリング)の裾野部の検出には固液界面検出に用いた高輝度帯の輝度ピーク部の値に所定の閾値割合乗算して求める。前記閾値割合は、70%以上90%以下の範囲であるのが好ましい。また、前記シリコン単結晶の直径制御は、前記シリコン単結晶の引上速度および前記シリコン融液の温度を、それぞれ制御することによって行えばよい。
具体的には、前記メニスカス高さを直径変化が0となる高さに引き上げ速度、およびヒータ温度を制御する。制御方法はPID制御が一般的であるが、その他の手法でもかまわない。ここで目標となるメニスカス高さが必要となるが、その目標メニスカス高さは事前にテストを行い、直径変動が0となるメニスカス高さを求めておく。
The meniscus height may be a difference between the liquid surface position and the solid-liquid interface position.
Specifically, the solid-liquid interface position is obtained from the center position calculated by circularly approximating the position at the luminance peak portion of the high luminance band (fusion ring), and the liquid surface position is the luminance of the high luminance band (fusion ring). The position at the skirt part on the melt side from the peak part is obtained from the center position calculated by circular approximation. The meniscus height is the difference between the two. The detection of the base part of the high luminance band (fusion ring) necessary for calculating the liquid surface position is obtained by multiplying the value of the luminance peak part of the high luminance band used for solid-liquid interface detection by a predetermined threshold ratio. The threshold ratio is preferably in the range of 70% to 90%. The diameter control of the silicon single crystal may be performed by controlling the pulling speed of the silicon single crystal and the temperature of the silicon melt.
Specifically, the meniscus height is increased to a height at which the diameter change becomes 0, and the heater temperature is controlled. The control method is generally PID control, but other methods may be used. Here, the target meniscus height is required, but the target meniscus height is tested in advance to obtain the meniscus height at which the diameter variation is zero.
引き上げ中に炉内をカメラで測定する場合、カメラは斜め上方より炉内を撮影することとなり、カメラ画角の影響で結晶中心部の固液界面は隠される。そのため、結晶中心部付近では高輝度帯全体を観察することは困難である。本発明では、前記液面位置と前記固液界面位置を測定の際に用いる前記シリコン高輝度帯の範囲を引き上げ中の結晶の中心より所定の距離だけ手前にある高輝度帯データに限定することができる。測定時に設定する所定の距離はカメラ設置条件、レンズの焦点距離等の光学条件、および測定対象の結晶の大きさ、形状により決定される。実際には前記条件で決定された距離にオフセットを加えた値に設定することが好ましく、その値は10mm程度がよい。これにより、前記液面位置と前記固液界面位置との測定精度を向上することが可能となる。なお、上記の範囲外だと、前記液面位置と前記固液界面位置とを正確に測定することが難しくなるので、好ましくない。 When the inside of the furnace is measured with a camera during the pulling, the camera takes an image of the inside of the furnace from obliquely above, and the solid-liquid interface at the center of the crystal is hidden by the influence of the camera angle of view. For this reason, it is difficult to observe the entire high luminance band in the vicinity of the center of the crystal. In the present invention, the range of the silicon high-intensity band used when measuring the liquid surface position and the solid-liquid interface position is limited to high-intensity band data that is a predetermined distance before the center of the crystal being pulled up. Can do. The predetermined distance set at the time of measurement is determined by camera installation conditions, optical conditions such as the focal length of the lens, and the size and shape of the crystal to be measured. Actually, it is preferable to set a value obtained by adding an offset to the distance determined under the above conditions, and the value is preferably about 10 mm. Thereby, it becomes possible to improve the measurement accuracy of the liquid surface position and the solid-liquid interface position. In addition, if it is outside the above range, it is difficult to accurately measure the liquid surface position and the solid-liquid interface position, which is not preferable.
また、カメラで直径測定する場合、その測定対象までの距離が変動するとその見かけの大きさが変化する。前記見かけの大きさから実際の大きさに換算する際は測定対象までの距離をもとに補正は可能であるが、そのためにはその距離変化を測定する必要がある。本発明では、前記液面位置をもとに、前記ルツボの位置を所定位置に制御することで前記液面位置を制御することができ、これにより、メニスカス高さ測定値への液面位置変化の影響を除去することが可能となる。通常前記の所定位置は結晶の引き上げ条件で決定される値であり、引き上げ中に一定である必要は無い。 Also, when measuring the diameter with a camera, the apparent size changes when the distance to the measurement object fluctuates. When converting from the apparent size to the actual size, correction is possible based on the distance to the object to be measured. To that end, it is necessary to measure the distance change. In the present invention, the liquid surface position can be controlled by controlling the position of the crucible to a predetermined position based on the liquid surface position, thereby changing the liquid surface position to the meniscus height measurement value. Can be removed. Usually, the predetermined position is a value determined by the crystal pulling condition and does not have to be constant during the pulling.
本発明のシリコン単結晶引上方法によれば、シリコン単結晶の直径制御に、高輝度帯(フュージョンリング)より算出される液面位置と固液界面位置の差分となるメニスカス高さを利用することにより、シリコン単結晶の直径が予め設定した規定値よりも大幅にズレてしまう前に、シリコン単結晶の直径が予め設定した規定値内に収まるように、シリコン単結晶の引上速度およびシリコン融液の温度など、シリコン単結晶の直径制御に係る手段に対して、迅速にフィードバックすることが可能になる。また、本発明にて同時に検出される液面位置をもとに液面位置を所望の高さに制御することが可能となる。これにより、所望の液面位置で、直胴部の直径が一定に保たれた、結晶欠陥の少ない高品質なシリコン単結晶を得ることが可能になる。 According to the silicon single crystal pulling method of the present invention, the meniscus height, which is the difference between the liquid surface position calculated from the high luminance band (fusion ring) and the solid-liquid interface position, is used for the diameter control of the silicon single crystal. As a result, the pulling speed of the silicon single crystal and the silicon are adjusted so that the diameter of the silicon single crystal falls within the predetermined specified value before the diameter of the silicon single crystal greatly deviates from the predetermined specified value. It is possible to provide quick feedback to the means related to the diameter control of the silicon single crystal, such as the temperature of the melt. In addition, the liquid surface position can be controlled to a desired height based on the liquid surface position detected simultaneously in the present invention. This makes it possible to obtain a high-quality silicon single crystal with few crystal defects, in which the diameter of the straight body portion is kept constant at a desired liquid level position.
以下、本発明に係るシリコン単結晶引上方法の最良の実施形態について、図面に基づき説明する。なお、本実施形態は発明の趣旨をより良く理解させるために具体的に説明するものであり、特に指定のない限り、本発明を限定するものではない。 The best mode for carrying out a silicon single crystal pulling method according to the present invention will be described below with reference to the drawings. In addition, this embodiment is specifically described in order to make the gist of the invention better understood, and does not limit the present invention unless otherwise specified.
図1は、チョクラルスキー法によってシリコン単結晶を引上る(育成する)様子を示した説明図である。シリコン単結晶の引上にあたっては、単結晶引上装置10を構成する、例えば石英からなるルツボ11にポリシリコンを投入し、ルツボ11を取り巻くように配されたヒータ12によってルツボ11を加熱する。そして、ポリシリコンを溶融し、ルツボ11内にシリコン融液13を形成する(溶融工程)。
FIG. 1 is an explanatory view showing a state in which a silicon single crystal is pulled (grown) by the Czochralski method. When pulling up the silicon single crystal, polysilicon is charged into a
次に、種結晶をシリコン融液13に接触させ、所定の回転速度で回転させつつ、直径を漸増させたショルダー部15aを形成し、続いて、予め設定した所定の直径を保った直胴部15bを育成し、所定の長さのシリコン単結晶15を得る。
Next, the
このようなシリコン単結晶15の育成にあたって、直胴部15bの直径を一定に保ちつつ引上ることは、結晶欠陥の少ない高品質なシリコン単結晶を得るために重要である。本発明のシリコン単結晶引上方法では、シリコン単結晶15の引上(育成)時に、シリコン融液13とシリコン単結晶15との固液界面近傍に生じる高輝度帯(フュージョンリング)FRの輝度を、輝度測定手段16によって測定する。
In growing such a silicon
この高輝度帯(フュージョンリング)FRは、引上中のシリコン単結晶の表面張力により持ち上がったシリコン融液の表面に、ルツボ壁からの放射光が反射して、固液界面でシリコン単結晶を取り巻く環状の高輝度領域が形成されたものである。 This high-intensity band (fusion ring) FR reflects the radiated light from the crucible wall to the surface of the silicon melt lifted by the surface tension of the silicon single crystal being pulled up, so that the silicon single crystal is formed at the solid-liquid interface. An annular high brightness region is formed.
本発明においては、シリコン単結晶15の育成中、輝度測定手段16によって継続して高輝度帯(フュージョンリング)FRの輝度を測定する。測定にあたっては、画像中の水平方向での高輝度帯(フュージョンリング)FRの輝度分布を測定する。そして、得られた高輝度帯(フュージョンリング)FRの輝度分布に基づいて、シリコン融液13の液面位置と、固液界面位置とをそれぞれ検出する。
In the present invention, while the silicon
輝度測定手段16によって測定された高輝度帯(フュージョンリング)FRの輝度分布は、例えば、図2の右側に示すグラフのようになる。即ち、高輝度帯(フュージョンリング)FRの輝度のピークは、シリコン単結晶15の固液界面、高輝度帯(フュージョンリング)FRの輝度の裾野部分は、シリコン融液13が傾いている部分に相当することがわかる。そのため高輝度帯(フュージョンリング)FRのピーク輝度部を用いて算出された近似円の中心位置は、シリコン単結晶の固液界面の位置、一方、高輝度帯(フュージョンリング)FRの裾野部のデータを用いて算出した場合は、固液界面より下の融液部の位置を検出することになる。
The luminance distribution of the high luminance band (fusion ring) FR measured by the luminance measuring means 16 is, for example, as shown in the graph on the right side of FIG. That is, the luminance peak of the high-intensity band (fusion ring) FR is at the solid-liquid interface of the silicon
そして、シリコン単結晶15の引上中に、直胴部15bの直径が変化すると、結晶の固液界面の位置は変化する。例えば、引上中のシリコン単結晶の直径が減少しはじめると、それに対応して固液界面の位置が降下する。その時、高輝度帯(フュージョンリング)FRは、図3に示すように、輝度のピーク位置が変化する。高輝度帯(フュージョンリング)FRの輝度ピーク位置では、シリコン単結晶の直径が変動する際の固液界面の位置が反映される。これにより、高輝度帯(フュージョンリング)FRの輝度の測定結果を用いて算出された近似円の中心位置は、シリコン結晶の直径変動時における、固液界面高さの変動を反映した結果が得られる。
When the diameter of the
以上のように、輝度測定手段16によって高輝度帯(フュージョンリング)FRの、シリコン単結晶を引上方向に沿った輝度分布を測定し、測定した輝度分布に基づいて、シリコン融液の液面位置と、固液界面位置とをそれぞれ検出する。そして、液面位置と固液界面位置との差分であるメニスカス高さの変動を連続して監視(測定)することによって、シリコン単結晶の直径が変動し始める兆候をいち早く検知して、シリコン単結晶の直径制御を迅速、かつ確実に行うことが可能になる。 As described above, the luminance measurement means 16 measures the luminance distribution along the pulling direction of the silicon single crystal in the high luminance band (fusion ring) FR, and based on the measured luminance distribution, the liquid surface of the silicon melt The position and the solid-liquid interface position are detected. Then, by continuously monitoring (measuring) the fluctuation of the meniscus height, which is the difference between the liquid surface position and the solid-liquid interface position, the signs of the silicon single crystal starting to fluctuate are quickly detected, and the silicon single crystal is detected. It becomes possible to control the diameter of the crystal quickly and reliably.
このように、シリコン単結晶の直径制御に、高輝度帯(フュージョンリング)FRの、シリコン単結晶を引上方向に沿った輝度分布を利用する方法は、従来のような、境界が明瞭でない高輝度帯(フュージョンリング)の幅や直径の変動を検出する方法と比較して、引上中のシリコン単結晶の直径の変化を正確、かつ迅速に検出することができる。 As described above, the method of using the luminance distribution along the pulling-up direction of the silicon single crystal in the high-luminance band (fusion ring) FR for controlling the diameter of the silicon single crystal has a high boundary where the boundary is not clear. Compared with a method for detecting variations in the width and diameter of a luminance band (fusion ring), a change in the diameter of a silicon single crystal during pulling can be detected accurately and rapidly.
よって、シリコン単結晶の直径が予め設定した規定値よりも大幅にズレてしまう前に、シリコン単結晶の直径が予め設定した規定値内に収まるように、シリコン単結晶の引上速度およびシリコン融液の温度など、シリコン単結晶の直径制御に係る手段に対して、迅速にフィードバックすることが可能になる。これにより、直胴部15bの直径が一定に保たれた、結晶欠陥の少ない高品質なシリコン単結晶を得ることが可能になる。
Therefore, before the diameter of the silicon single crystal is significantly deviated from the preset specified value, the pulling speed of the silicon single crystal and the silicon melt are adjusted so that the diameter of the silicon single crystal is within the preset specified value. It is possible to provide quick feedback to means relating to the diameter control of the silicon single crystal, such as the temperature of the liquid. This makes it possible to obtain a high-quality silicon single crystal with few crystal defects, in which the diameter of the
図4は、実際の単結晶引上装置で測定した、シリコン単結晶の直径、直径変化量(直径微分値)、およびシリコン融液のメニスカス高さの測定結果を示すグラフである。図4に示した結果から、シリコン単結晶の直径変化量とメニスカス高さとは、逆位相で非常に高く一致する傾向を示した。 FIG. 4 is a graph showing measurement results of the silicon single crystal diameter, diameter change (diameter differential value), and silicon melt meniscus height measured with an actual single crystal pulling apparatus. From the results shown in FIG. 4, it was found that the amount of change in diameter of the silicon single crystal and the meniscus height tended to be very high in antiphase.
図5は、図4に示したシリコン単結晶の直径変化量と、メニスカス高さとの相関を示す分布図である。この図5からも、引上中のシリコン単結晶の直径が増加し始める際には、メニスカス高さが減少し、逆に、直径が減少し始める際には、メニスカス高さが増加することが確認された。 FIG. 5 is a distribution diagram showing the correlation between the change in diameter of the silicon single crystal shown in FIG. 4 and the meniscus height. Also from FIG. 5, when the diameter of the silicon single crystal being pulled starts to increase, the meniscus height decreases, and conversely, when the diameter starts to decrease, the meniscus height increases. confirmed.
従来、単結晶引上装置における単結晶の直径制御は、直径値を入力し、実際に測定した直径値の目標値からのズレに基づき、PIDにて引き上げ速度およびヒータ温度を制御することにより直径制御を行っている。しかし、現状のようにシリコン単結晶が大口径化し、初期のポリシリコンの投入量が増大すると、引上時の直径制御が困難となる。
そこで直径の測定値に代えて直径変化量を入力、即ち直径変化量を目標値(直胴部では0)にするように制御することによって、従来の直径制御よりも早いタイミングでの操作が可能なり、直径制御性の向上を図ることができるとされていた。
Conventionally, the diameter control of the single crystal in the single crystal pulling apparatus is performed by inputting the diameter value and controlling the pulling speed and the heater temperature with the PID based on the deviation of the actually measured diameter value from the target value. Control is in progress. However, when the diameter of the silicon single crystal is increased as in the present situation and the initial amount of polysilicon is increased, it becomes difficult to control the diameter during pulling.
Therefore, it is possible to operate at a timing earlier than the conventional diameter control by inputting the diameter change amount instead of the measured diameter value, that is, by controlling the diameter change amount to be the target value (0 in the case of the straight body portion). Therefore, it was said that the diameter controllability could be improved.
しかしながら、図4に示したグラフからも分かるように、実際に制御に適用可能なレベルの直径変化量を算出するためには、移動平均などを用いたSNの向上が必須であり、そのため直径変化量を用いたことによって得られる、迅速なタイミングでの直径制御による効果は相殺されてしまう。 However, as can be seen from the graph shown in FIG. 4, in order to calculate the amount of change in diameter at a level that can be actually applied to control, it is essential to improve SN using a moving average or the like. The effect of diameter control at a quick timing obtained by using the quantity is offset.
一方、本発明においては、メニスカス高さは移動平均なしの値にも関わらず、シリコン単結晶の直径変化量の結果とほぼ同等のSNを確保しており、移動平均等の処置は必要ない。そのため、メニスカス高さを用いた直径制御によりも早いタイミングでの直径制御のための操作が実現可能となり、直径制御性を大きく改善することが可能になる。 On the other hand, in the present invention, although the meniscus height is a value without a moving average, an SN substantially equal to the result of the diameter change amount of the silicon single crystal is secured, and a treatment such as a moving average is not necessary. Therefore, an operation for controlling the diameter at an earlier timing can be realized than the diameter control using the meniscus height, and the diameter controllability can be greatly improved.
こうしたメニスカス高さに基づいた直径制御においては、目標となるメニスカス高さは図5に示すような、直径変化に対する相関解析に基づいて設定する。例えば、図4に示すグラフの場合、目標となるメニスカス高さは2.5mmあり、メニスカス高さ2.5mmでの直径変化量は0mmであるため、シリコン単結晶の直胴部は、メニスカス高さを2.5mmなるように、メニスカス高さをもとにPID演算によって、引上速度、ヒータ温度(シリコン融液温度)を制御すればよい。 In the diameter control based on the meniscus height, the target meniscus height is set based on the correlation analysis with respect to the diameter change as shown in FIG. For example, in the case of the graph shown in FIG. 4, the target meniscus height is 2.5 mm, and the diameter variation at the meniscus height of 2.5 mm is 0 mm. The pulling speed and heater temperature (silicon melt temperature) may be controlled by PID calculation based on the meniscus height so that the thickness is 2.5 mm.
図5から、メニスカス高さと直径変化とは傾き−0.08の比例関係にありその相関係数は0.8以上となることがわかる。ここからメニスカス高さと直径変化との関係はy=−0.08x+0.2で表される。つまり、この相関関係に基づいて、メニスカス高さの変化に対応して、引上速度、ヒータ温度を制御することができる。
そして、メニスカス高さが上昇した場合は、引き上げ速度を低下もしくはヒータ温度低下、逆にメニスカス高さが低下した場合は、引き上げ速度を増加もしくはヒータ温度上昇させる操作を行うこととする。
From FIG. 5, it can be seen that the meniscus height and the diameter change have a proportional relationship of slope -0.08, and the correlation coefficient is 0.8 or more. From this, the relationship between meniscus height and diameter change is expressed as y = −0.08x + 0.2. That is, based on this correlation, the pulling speed and the heater temperature can be controlled in accordance with the change in meniscus height.
When the meniscus height is increased, the pulling speed is decreased or the heater temperature is decreased. Conversely, when the meniscus height is decreased, the pulling speed is increased or the heater temperature is increased.
メニスカス高さを算出する際にシリコン融液の液面位置を示す高輝度帯(フュージョンリング)FRのエッジ部の設定は、高輝度帯(フュージョンリング)の輝度分布を測定して得られた輝度ピーク値に対して、所定の閾値割合を乗算して求めた輝度閾値であればよい。例えば、図6に示すグラフのように、高輝度帯(フュージョンリング)の輝度ピーク値に対して、閾値割合を90%に設定し、この閾値割合を90%とした横線と輝度分布を示す連続線との交点を輝度閾値、即ち、シリコン融液の液面位置を示す値として用いればよい。なお、この閾値割合は、輝度ピーク値に対して70〜95%、例えば、90%であればよい。 When calculating the meniscus height, the setting of the edge portion of the high luminance band (fusion ring) FR indicating the position of the silicon melt surface is obtained by measuring the luminance distribution of the high luminance band (fusion ring). Any luminance threshold value obtained by multiplying the peak value by a predetermined threshold ratio may be used. For example, as shown in the graph of FIG. 6, the threshold ratio is set to 90% with respect to the luminance peak value in the high luminance band (fusion ring), and the horizontal line and the luminance distribution with the threshold ratio set to 90% are shown. The intersection with the line may be used as a luminance threshold value, that is, a value indicating the liquid surface position of the silicon melt. The threshold ratio may be 70 to 95%, for example, 90% with respect to the luminance peak value.
10 単結晶引上装置、11 ルツボ、13 シリコン融液、15 シリコン単結晶、16 輝度検出手段。
10 single crystal pulling device, 11 crucible, 13 silicon melt, 15 silicon single crystal, 16 luminance detection means.
Claims (4)
前記引上工程において、撮像装置を用いて前記シリコン単結晶を撮像し、該撮像装置で撮像した画像中の前記シリコン融液と前記シリコン単結晶との固液界面近傍に生じる高輝度帯の輝度分布を各画像走査線毎に測定し、前記シリコン融液の液面位置と、前記固液界面位置とをそれぞれ検出する工程と、
前記液面位置と前記固液界面位置との差分であるメニスカス高さに基づいて、前記シリコン単結晶の直径制御を行う工程とを備え、
前記メニスカス高さは、前記画像中の固液界面近傍に生じる高輝度帯の前記各走査線毎の輝度分布において輝度が最も高い輝度ピーク部での検出位置を円近似し算出した中心位置による固液界面位置と、前記輝度ピーク部に対して前記シリコン融液側の輝度分布裾野部での位置を円近似し算出した中心位置による液面位置との差分であり、
前記液面位置を算出する際の輝度分布の裾野部分を前記輝度ピーク部の値に所定の閾値割合を乗算して求めた輝度閾値を用いて検出された位置とし、前記閾値割合は、70%以上90%以下の範囲であることを特徴とするシリコン単結晶引上方法。 A silicon single crystal pulling method comprising: a melting step of melting polycrystalline silicon contained in a crucible to form a silicon melt in the crucible; and a pulling step of pulling up the silicon single crystal from the silicon melt by the Czochralski method. The above method,
In the pulling-up step, the silicon single crystal is imaged using an imaging device, and the brightness of a high-luminance zone generated in the vicinity of the solid-liquid interface between the silicon melt and the silicon single crystal in the image captured by the imaging device Measuring the distribution for each image scanning line, and detecting each of the liquid surface position of the silicon melt and the solid-liquid interface position;
A step of controlling the diameter of the silicon single crystal based on a meniscus height which is a difference between the liquid surface position and the solid-liquid interface position;
The meniscus height is a fixed value based on the center position calculated by circularly approximating the detection position at the luminance peak portion where the luminance is highest in the luminance distribution for each scanning line in the high luminance band generated near the solid-liquid interface in the image. The difference between the liquid interface position and the liquid surface position by the center position calculated by circularly approximating the position at the luminance distribution skirt part on the silicon melt side with respect to the luminance peak part,
The base part of the luminance distribution at the time of calculating the liquid surface position is a position detected by using a luminance threshold value obtained by multiplying the value of the luminance peak part by a predetermined threshold ratio, and the threshold ratio is 70% features and to Resid silicon single crystal pulling method to be a range of 90% or less.
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